CN106242007A - A kind of preparation method of copper-containing residue solid ozone Composite denitrification agent - Google Patents
A kind of preparation method of copper-containing residue solid ozone Composite denitrification agent Download PDFInfo
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- CN106242007A CN106242007A CN201610595545.0A CN201610595545A CN106242007A CN 106242007 A CN106242007 A CN 106242007A CN 201610595545 A CN201610595545 A CN 201610595545A CN 106242007 A CN106242007 A CN 106242007A
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- copper
- containing residue
- denitrifier
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/58—Treatment of water, waste water, or sewage by removing specified dissolved compounds
- C02F1/586—Treatment of water, waste water, or sewage by removing specified dissolved compounds by removing ammoniacal nitrogen
Abstract
The present invention relates to the preparation method of a kind of copper-containing residue solid ozone Composite denitrification agent, belong to denitrifier preparation field.For current high-concentration ammonia nitrogenous wastewater in governance process, chemistry room and Biochemical method cost are high, investment is big, bioanalysis is to the poor problem of the treatment effect of ammonia nitrogen, by copper-containing residue being milled and dispersed ultrafine modification copper-containing residue is prepared in modification, the most synthetically prepared cupric denitrifier, by preparing Composite denitrification agent granule by cupric denitrifier in ozone gas freezing, by copper and NH3·H2O forms Metal amine complex, simultaneously under ozone catalytic effect, improve its to high concentration wastewater treatment efficiency, ammonia nitrogen removal frank is up to 80%；Denitrifier, environmental protection non-secondary pollution is prepared by copper-containing residue powder.
Description
Technical field
The present invention relates to the preparation method of a kind of copper-containing residue solid ozone Composite denitrification agent, belong to denitrifier preparation neck
Territory.
Background technology
Ammonia nitrogen in water refers to the nitrogen existed with free ammonia and ion ammonia form, and being mainly derived from nitrogenous in sanitary sewage has
In the water bodys such as the decomposition of machine thing, coking, the synthesis industrial wastewater such as ammonia, and agricultural drain, the ammonia nitrogen of high-load can cause surface water
Eutrophication, causes the biological amount reproductions such as pasture and water cyanophyceae, affects water quality, and ammonia nitrogen presents toxic action to Fish, to human body also
Having harm in various degree, not only ammonia nitrogen has toxicity, and its oxidation product nitrite nitrogen has toxicity, equally such as low concentration
Nitrite nitrogen can make the resistance of cultivated animals reduce, and easily infects various diseases, and erythrocyte can be destroyed, make blood
Oxygen delivery capacity is gradually lost, and it is also easy to cause the function of the liver spleen of animal and kidney the most evident in addition, causes flag, essence
God is the best.
During existing process high-concentration ammonia nitrogenous wastewater, mainly there are chemical method and biology side for the processing method of ammonia nitrogen in waste water
Method, although they can play a significant role in water processes, but several method processing cost is high, and investment is big, and bioanalysis is to ammonia
The treatment effect of nitrogen is poor, and many ammonia nitrogen in industrial waste waters is dense, and these waste water is difficult to or at all can not be with often
The bioanalysis of rule is removed and NH3·H2O can form more stable Metal amine complex with transition metal copper so that ammonia nitrogen obtains
Separate and remove.So needing the denitrifier of a kind of recycling necessary.
Summary of the invention
The technical problem that present invention mainly solves: for current high-concentration ammonia nitrogenous wastewater in governance process, chemistry room and
Biochemical method cost is high, and investment is big, and bioanalysis is to the poor problem of the treatment effect of ammonia nitrogen, it is provided that a kind of by by cupric
Waste residue is milled and dispersed ultrafine modification copper-containing residue is prepared in modification, and the most synthetically prepared cupric denitrifier, by taking off cupric
Nitrogen agent prepares Composite denitrification agent granule in ozone gas freezing, by copper and NH3·H2O forms Metal amine complex, simultaneously smelly
Under oxygen catalytic action, accelerated oxidation and reaction rate, improve it to high-concentration ammonia nitrogenous wastewater efficiency.
In order to solve above-mentioned technical problem, the technical solution adopted in the present invention:
(1) choose copper-containing residue, by it as grinding under 10～15MPa and sieving, be prepared into the copper-containing residue of 80～90 mesh, press
Parts by weight meter, weighs the copper-containing residue of 35～55 parts of above-mentioned preparations, 15～20 parts of sodium hydroxide and 30～45 parts of distillations respectively
Water, in beaker, is stirred for mixing and as heating in water bath 2～3h at 95～100 DEG C；
(2) to be heated complete after, it is processed 10～15min as ultrasonic disperse under 200～300W, then 1800～2000r/
Centrifugal reaction 10～15min under min, collects precipitation next time subsequently, is washed with deionized 3～5 times, and dry at 65～80 DEG C
Dry 6～8h, it is prepared into modified copper-containing residue powder；
(3) count by weight, weigh 45～60 parts of deionized waters, 15～20 parts of sodium hydroxide, 15～20 parts of above-mentioned systems respectively
Standby modified copper-containing residue powder and 10～15 parts of sodium silicate are in there-necked flask, and stirring mixing is also incubated at 55～65 DEG C
Reacting by heating 3～5h；
(4) after question response completes, its intensification is heated to 95～100 DEG C so that it is crystallization 5～8h, after crystallization completes, uses
The sodium hydroxide solution regulation pH to 8.5～9.0 of 0.8mol/L, is stood subsequently and is cooled to 20～30 DEG C, filtered it also
Collect filtering residue, at 95～100 DEG C, be dried 20～24h, be prepared into cupric denitrifier；(5) by the cupric denitrifier of above-mentioned preparation
As for milling under 10～15MPa and sieving, it is prepared into 120～150 purpose ultra-fine cupric denitrifier, containing above-mentioned preparation subsequently
Copper granule denitrifier and ozone, in jet-impingement to liquid nitrogen freezing device, make denitrifier granule mixing ozone freezing processing, i.e.
A kind of copper-containing residue solid ozone Composite denitrification agent can be prepared into.
The application of the present invention: 0.06g/mL is pressed in the copper-containing residue solid ozone Composite denitrification agent of foregoing invention, 20～
At 30 DEG C, putting in high-concentration waste water, controlling stirring waste water speed is 200～250r/min, and ammonia nitrogen is gone by 20min to be added
Except rate is up to 80%.
The invention has the beneficial effects as follows: (1) present invention, by under solid ozone catalytic effect, improves it to high-concentration waste
Water treatment efficiency, is up to 80% to ammonia nitrogen removal frank；
(2) denitrifier, environmental protection non-secondary pollution are prepared by copper-containing residue powder.
Detailed description of the invention
Selecting and choose copper-containing residue, by it as grinding under 10～15MPa and sieving, the cupric being prepared into 80～90 mesh gives up
Slag, counts by weight, weighs the copper-containing residue of 35～55 parts of above-mentioned preparations, 15～20 parts of sodium hydroxide and 30～45 parts respectively
Distilled water, in beaker, is stirred for mixing and as heating in water bath 2～3h at 95～100 DEG C；To be heated complete after, by it extremely
Under 200～300W, ultrasonic disperse processes 10～15min, more centrifugal reaction 10～15min under 1800～2000r/min, with
Rear collection is precipitated next time, is washed with deionized 3～5 times, and is dried 6～8h at 65～80 DEG C, is prepared into modified cupric and gives up
Ground-slag end；Count by weight, weigh 45～60 parts of deionized waters, 15～20 parts of sodium hydroxide, 15～20 parts of above-mentioned systems respectively
Standby modified copper-containing residue powder and 10～15 parts of sodium silicate are in there-necked flask, and stirring mixing is also incubated at 55～65 DEG C
Reacting by heating 3～5h；After question response completes, its intensification is heated to 95～100 DEG C so that it is crystallization 5～8h, treats that crystallization completes
After, regulate pH to 8.5～9.0 with the sodium hydroxide solution of 0.8mol/L, stood subsequently and be cooled to 20～30 DEG C, to its mistake
Filter and collect filtering residue, at 95～100 DEG C, being dried 20～24h, be prepared into cupric denitrifier；By the cupric denitrifier of above-mentioned preparation
As for milling under 10～15MPa and sieving, it is prepared into 120～150 purpose ultra-fine cupric denitrifier, containing above-mentioned preparation subsequently
Copper granule denitrifier and ozone, in jet-impingement to liquid nitrogen freezing device, make denitrifier granule mixing ozone freezing processing, i.e.
A kind of copper-containing residue solid ozone Composite denitrification agent can be prepared into.
Example 1
Select and choose copper-containing residue, by it as grinding under 10MPa and sieving, be prepared into the copper-containing residue of 80 mesh, by weight
Number meter, weighs the copper-containing residue of 35 parts of above-mentioned preparations respectively, and 20 parts of sodium hydroxide and 45 parts of distilled water, in beaker, are stirred for
Mixing as heating in water bath 2h at 95 DEG C；To be heated complete after, by its as under 200W ultrasonic disperse process 10min, then
Under 1800r/min, centrifugal reaction 10min, collects precipitation next time subsequently, is washed with deionized 3 times, and is dried 6h at 65 DEG C,
It is prepared into modified copper-containing residue powder；Count by weight, weigh respectively 45 parts of deionized waters, 20 parts of sodium hydroxide, on 20 parts
State the modified copper-containing residue powder of preparation and 15 parts of sodium silicate in there-necked flask, stirring mixing as Heat preservation at 55 DEG C
Reaction 3h；After question response completes, its intensification is heated to 95 DEG C so that it is crystallization 5h, after crystallization completes, with the hydrogen of 0.8mol/L
Sodium hydroxide solution regulation pH to 8.5, is stood subsequently and is cooled to 20 DEG C, filter it and collect filtering residue, be dried at 95 DEG C
20h, is prepared into cupric denitrifier；By the cupric denitrifier of above-mentioned preparation as milling under 10MPa and sieving, it is prepared into 120 mesh
Ultra-fine cupric denitrifier, subsequently by the cupric granule denitrifier of above-mentioned preparation and ozone through jet-impingement to liquid nitrogen freezing device
In, make denitrifier granule mixing ozone freezing processing, a kind of copper-containing residue solid ozone Composite denitrification agent can be prepared into.
0.06g/mL is pressed in the copper-containing residue solid ozone Composite denitrification agent of foregoing invention, at 20 DEG C, puts into high concentration
In waste water, controlling stirring waste water speed is 200r/min, and 20min to be added is up to 80% to ammonia nitrogen removal frank.
Example 2
Select and choose copper-containing residue, by it as grinding under 12MPa and sieving, be prepared into the copper-containing residue of 85 mesh, by weight
Number meter, weighs the copper-containing residue of 40 parts of above-mentioned preparations respectively, and 20 parts of sodium hydroxide and 40 parts of distilled water, in beaker, are stirred for
Mixing as heating in water bath 2h at 97 DEG C；To be heated complete after, by its as under 250W ultrasonic disperse process 13min, then
Under 1900r/min, centrifugal reaction 12min, collects precipitation next time subsequently, is washed with deionized 4 times, and is dried 7h at 70 DEG C,
It is prepared into modified copper-containing residue powder；Count by weight, weigh respectively 50 parts of deionized waters, 20 parts of sodium hydroxide, on 15 parts
State the modified copper-containing residue powder of preparation and 15 parts of sodium silicate in there-necked flask, stirring mixing as Heat preservation at 57 DEG C
Reaction 4h；After question response completes, its intensification is heated to 98 DEG C so that it is crystallization 6h, after crystallization completes, with the hydrogen of 0.8mol/L
Sodium hydroxide solution regulation pH to 8.7, is stood subsequently and is cooled to 25 DEG C, filter it and collect filtering residue, be dried at 97 DEG C
22h, is prepared into cupric denitrifier；By the cupric denitrifier of above-mentioned preparation as milling under 12MPa and sieving, it is prepared into 130 mesh
Ultra-fine cupric denitrifier, subsequently by the cupric granule denitrifier of above-mentioned preparation and ozone through jet-impingement to liquid nitrogen freezing device
In, make denitrifier granule mixing ozone freezing processing, a kind of copper-containing residue solid ozone Composite denitrification agent can be prepared into.
0.06g/mL is pressed in the copper-containing residue solid ozone Composite denitrification agent of foregoing invention, at 25 DEG C, puts into high concentration
In waste water, controlling stirring waste water speed is 225r/min, and 20min to be added is up to 80% to ammonia nitrogen removal frank.
Example 3
Select and choose copper-containing residue, by it as grinding under 15MPa and sieving, be prepared into the copper-containing residue of 90 mesh, by weight
Number meter, weighs the copper-containing residue of 55 parts of above-mentioned preparations respectively, and 15 parts of sodium hydroxide and 30 parts of distilled water, in beaker, are stirred for
Mixing as heating in water bath 3h at 100 DEG C；To be heated complete after, by its as under 300W ultrasonic disperse process 15min, then
Under 2000r/min, centrifugal reaction 15min, collects precipitation next time subsequently, is washed with deionized 5 times, and is dried 8h at 80 DEG C,
It is prepared into modified copper-containing residue powder；Count by weight, weigh respectively 60 parts of deionized waters, 15 parts of sodium hydroxide, on 15 parts
State the modified copper-containing residue powder of preparation and 10 parts of sodium silicate in there-necked flask, stirring mixing as Heat preservation at 65 DEG C
Reaction 5h；After question response completes, its intensification is heated to 100 DEG C so that it is crystallization 8h, after crystallization completes, with 0.8mol/L's
Sodium hydroxide solution regulation pH to 9.0, is stood subsequently and is cooled to 30 DEG C, filter it and collect filtering residue, dry at 100 DEG C
Dry 24h, is prepared into cupric denitrifier；By the cupric denitrifier of above-mentioned preparation as milling under 15MPa and sieving, it is prepared into 120
～150 purpose ultra-fine cupric denitrifier, subsequently by the cupric granule denitrifier of above-mentioned preparation and ozone through jet-impingement to liquid nitrogen
In refrigerating plant, make denitrifier granule mixing ozone freezing processing, a kind of copper-containing residue solid ozone can be prepared into compound de-
Nitrogen agent.
0.06g/mL is pressed in the copper-containing residue solid ozone Composite denitrification agent of foregoing invention, at 30 DEG C, puts into high concentration
In waste water, controlling stirring waste water speed is 250r/min, and 20min to be added is up to 80% to ammonia nitrogen removal frank.
Claims (1)
1. the preparation method of a copper-containing residue solid ozone Composite denitrification agent, it is characterised in that concrete preparation process is:
(1) choose copper-containing residue, by it as grinding under 10～15MPa and sieving, be prepared into the copper-containing residue of 80～90 mesh, press
Parts by weight meter, weighs the copper-containing residue of 35～55 parts of above-mentioned preparations, 15～20 parts of sodium hydroxide and 30～45 parts of distillations respectively
Water, in beaker, is stirred for mixing and as heating in water bath 2～3h at 95～100 DEG C；
(2) to be heated complete after, it is processed 10～15min as ultrasonic disperse under 200～300W, then 1800～2000r/
Centrifugal reaction 10～15min under min, collects precipitation next time subsequently, is washed with deionized 3～5 times, and dry at 65～80 DEG C
Dry 6～8h, it is prepared into modified copper-containing residue powder；
(3) count by weight, weigh 45～60 parts of deionized waters, 15～20 parts of sodium hydroxide, 15～20 parts of above-mentioned systems respectively
Standby modified copper-containing residue powder and 10～15 parts of sodium silicate are in there-necked flask, and stirring mixing is also incubated at 55～65 DEG C
Reacting by heating 3～5h；
(4) after question response completes, its intensification is heated to 95～100 DEG C so that it is crystallization 5～8h, after crystallization completes, uses
The sodium hydroxide solution regulation pH to 8.5～9.0 of 0.8mol/L, is stood subsequently and is cooled to 20～30 DEG C, filtered it also
Collect filtering residue, at 95～100 DEG C, be dried 20～24h, be prepared into cupric denitrifier；
(5) by the cupric denitrifier of above-mentioned preparation as milling under 10～15MPa and sieving, it is prepared into 120～150 purposes ultra-fine
Cupric denitrifier, subsequently by the cupric granule denitrifier of above-mentioned preparation and ozone in jet-impingement to liquid nitrogen freezing device, makes
Denitrifier granule mixing ozone freezing processing, can be prepared into a kind of copper-containing residue solid ozone Composite denitrification agent.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610595545.0A CN106242007A (en) | 2016-07-25 | 2016-07-25 | A kind of preparation method of copper-containing residue solid ozone Composite denitrification agent |
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| CN201610595545.0A CN106242007A (en) | 2016-07-25 | 2016-07-25 | A kind of preparation method of copper-containing residue solid ozone Composite denitrification agent |
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|---|---|---|---|---|
| JPS5248271A (en) * | 1975-10-14 | 1977-04-16 | Masakuni Kanai | Method of removing ammonia in water |
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| CN101792172A (en) * | 2010-03-03 | 2010-08-04 | 天津理工大学 | Method for preparing copper hydroxide and copper oxide nano material and application |
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| CN102390860A (en) * | 2011-08-04 | 2012-03-28 | 山东东岳有机硅材料有限公司 | Environmentally-friendly treatment method and device for organosilicon slurry |
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| CN103920454A (en) * | 2014-04-29 | 2014-07-16 | 哈尔滨理工大学 | Composite copper-based desulfurizing agent for removing sulfur-containing repugnant substances at normal temperature and preparation method of composite copper-based desulfurizing agent |
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2016
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| JPS5248271A (en) * | 1975-10-14 | 1977-04-16 | Masakuni Kanai | Method of removing ammonia in water |
| CN101792172A (en) * | 2010-03-03 | 2010-08-04 | 天津理工大学 | Method for preparing copper hydroxide and copper oxide nano material and application |
| CN101886179A (en) * | 2010-07-12 | 2010-11-17 | 昆明理工大学 | Method for separating ferrum, copper and silicon components from copper smelting residues |
| CN102390860A (en) * | 2011-08-04 | 2012-03-28 | 山东东岳有机硅材料有限公司 | Environmentally-friendly treatment method and device for organosilicon slurry |
| CN102614826A (en) * | 2012-03-27 | 2012-08-01 | 武汉科梦环境工程有限公司 | Modified expanded perlite for treating low-concentration ammonia-nitrogen wastewater and wastewater treatment method |
| CN104230073A (en) * | 2013-06-07 | 2014-12-24 | 欣兴电子股份有限公司 | Treatment method for ammonia-containing wastewater |
| CN103920454A (en) * | 2014-04-29 | 2014-07-16 | 哈尔滨理工大学 | Composite copper-based desulfurizing agent for removing sulfur-containing repugnant substances at normal temperature and preparation method of composite copper-based desulfurizing agent |
| CN105271503A (en) * | 2014-06-11 | 2016-01-27 | 蒋寿悟 | Method for enhanced removal of ammonia nitrogen in water through catalytic ozonation |
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